Dimethylcarbamoyl Chloride → 4-Dimethylcarbamoyloxy-2,5-dimethylphenyl methyl sulphide

HRID 27335ノート

反応式

HRID 27335 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([S:8][CH3:9])[C:5]([CH3:10])=[CH:4][C:3]=1[OH:11].[CH3:12][N:13]([CH3:17])[C:14](Cl)=[O:15]>N1C=CC=CC=1>[CH3:9][S:8][C:6]1[CH:7]=[C:2]([CH3:1])[C:3]([O:11][C:14](=[O:15])[N:13]([CH3:17])[CH3:12])=[CH:4][C:5]=1[CH3:10]

参加物

4

反応物 2

HCID 6598Dimethylcarbamoyl ChlorideHCID 12889671HCID 12889671、化合物

生成物 1

HCID 128896874-Dimethylcarbamoyloxy-2,5-dimethylphenyl methyl sulphide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
100 °C

実験手順

A mixture of 25.2 g 2,5-dimethyl-4-(methylthio)phenol and 20.3 ml dimethylcarbamoyl chloride in 70 ml dry pyridine was heated for 24 hours at 100° C. Addition to excess of ice-cold dilute hydrochloric acid gave an oil. The oil product was extracted into ether and washed three times with cold dilute sodium hydroxide and once with water, dried, and the ether removed by evaporation to give 4-dimethylcarbamoyloxy-2,5-dimethylphenyl methyl sulphide, boiling point 146° C. at 0.6 mm to 150° C. to 0.9 mm.

後処理

  1. additionAddition to excess of ice-cold dilute hydrochloric acid
  2. customgave an oil
  3. extractionThe oil product was extracted into ether
  4. washwashed three times with cold dilute sodium hydroxide
  5. dry with materialonce with water, dried
  6. customthe ether removed by evaporation

出典と根拠

ORDレコード
ord-7230bcee4b094bab8a059f5deb486c74
出典データセット
uspto-grants-1980_09
特許番号
US04221582

反応ノート

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